CN109160511A - A kind of device and method of graphite purification - Google Patents
A kind of device and method of graphite purification Download PDFInfo
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- CN109160511A CN109160511A CN201811083929.XA CN201811083929A CN109160511A CN 109160511 A CN109160511 A CN 109160511A CN 201811083929 A CN201811083929 A CN 201811083929A CN 109160511 A CN109160511 A CN 109160511A
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- graphite
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- bed reactor
- purification
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 115
- 229910002804 graphite Inorganic materials 0.000 title claims abstract description 111
- 239000010439 graphite Substances 0.000 title claims abstract description 111
- 238000000746 purification Methods 0.000 title claims abstract description 52
- 238000000034 method Methods 0.000 title claims abstract description 26
- 238000010438 heat treatment Methods 0.000 claims abstract description 48
- 239000002994 raw material Substances 0.000 claims abstract description 39
- 239000007787 solid Substances 0.000 claims abstract description 39
- 239000012535 impurity Substances 0.000 claims abstract description 15
- 239000007789 gas Substances 0.000 claims description 77
- 239000002912 waste gas Substances 0.000 claims description 46
- 238000009835 boiling Methods 0.000 claims description 31
- 238000011084 recovery Methods 0.000 claims description 27
- 150000001875 compounds Chemical class 0.000 claims description 23
- 150000002500 ions Chemical class 0.000 claims description 18
- 239000002904 solvent Substances 0.000 claims description 17
- 239000011261 inert gas Substances 0.000 claims description 14
- 238000003860 storage Methods 0.000 claims description 10
- 230000006698 induction Effects 0.000 claims description 8
- 238000004064 recycling Methods 0.000 claims description 4
- 150000008044 alkali metal hydroxides Chemical class 0.000 claims description 3
- 238000007664 blowing Methods 0.000 claims description 3
- 238000001035 drying Methods 0.000 claims description 3
- 229910000288 alkali metal carbonate Inorganic materials 0.000 claims description 2
- 150000008041 alkali metal carbonates Chemical class 0.000 claims description 2
- 238000004062 sedimentation Methods 0.000 claims 1
- 238000006243 chemical reaction Methods 0.000 abstract description 21
- 238000005265 energy consumption Methods 0.000 abstract description 12
- 238000003723 Smelting Methods 0.000 abstract description 4
- 239000000047 product Substances 0.000 description 18
- 238000001914 filtration Methods 0.000 description 11
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 5
- 229910052782 aluminium Inorganic materials 0.000 description 5
- 229910052742 iron Inorganic materials 0.000 description 5
- 229910052708 sodium Inorganic materials 0.000 description 5
- 239000000126 substance Substances 0.000 description 5
- 229910052791 calcium Inorganic materials 0.000 description 4
- 229910052749 magnesium Inorganic materials 0.000 description 4
- 229910021382 natural graphite Inorganic materials 0.000 description 4
- 229910052700 potassium Inorganic materials 0.000 description 4
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 description 3
- 239000002253 acid Substances 0.000 description 3
- 239000003513 alkali Substances 0.000 description 3
- 230000008901 benefit Effects 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 2
- TWRXJAOTZQYOKJ-UHFFFAOYSA-L Magnesium chloride Chemical compound [Mg+2].[Cl-].[Cl-] TWRXJAOTZQYOKJ-UHFFFAOYSA-L 0.000 description 2
- 229910001854 alkali hydroxide Inorganic materials 0.000 description 2
- 229910052783 alkali metal Inorganic materials 0.000 description 2
- 150000001340 alkali metals Chemical class 0.000 description 2
- VSCWAEJMTAWNJL-UHFFFAOYSA-K aluminium trichloride Chemical compound Cl[Al](Cl)Cl VSCWAEJMTAWNJL-UHFFFAOYSA-K 0.000 description 2
- 230000005540 biological transmission Effects 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 239000000460 chlorine Substances 0.000 description 2
- 229910052801 chlorine Inorganic materials 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000007770 graphite material Substances 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 229910052814 silicon oxide Inorganic materials 0.000 description 2
- UXVMQQNJUSDDNG-UHFFFAOYSA-L Calcium chloride Chemical compound [Cl-].[Cl-].[Ca+2] UXVMQQNJUSDDNG-UHFFFAOYSA-L 0.000 description 1
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 description 1
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 1
- 229910021578 Iron(III) chloride Inorganic materials 0.000 description 1
- 229910003910 SiCl4 Inorganic materials 0.000 description 1
- 229910003822 SiHCl3 Inorganic materials 0.000 description 1
- 241001062472 Stokellia anisodon Species 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000003139 buffering effect Effects 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 239000001110 calcium chloride Substances 0.000 description 1
- 229910001628 calcium chloride Inorganic materials 0.000 description 1
- BVKZGUZCCUSVTD-UHFFFAOYSA-N carbonic acid Chemical compound OC(O)=O BVKZGUZCCUSVTD-UHFFFAOYSA-N 0.000 description 1
- 239000012159 carrier gas Substances 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 239000012141 concentrate Substances 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000005243 fluidization Methods 0.000 description 1
- 238000002309 gasification Methods 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 229910000040 hydrogen fluoride Inorganic materials 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 description 1
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 229910001629 magnesium chloride Inorganic materials 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000005272 metallurgy Methods 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 230000009257 reactivity Effects 0.000 description 1
- 238000009938 salting Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 231100000004 severe toxicity Toxicity 0.000 description 1
- FDNAPBUWERUEDA-UHFFFAOYSA-N silicon tetrachloride Chemical compound Cl[Si](Cl)(Cl)Cl FDNAPBUWERUEDA-UHFFFAOYSA-N 0.000 description 1
- SUKJFIGYRHOWBL-UHFFFAOYSA-N sodium hypochlorite Chemical compound [Na+].Cl[O-] SUKJFIGYRHOWBL-UHFFFAOYSA-N 0.000 description 1
- 239000004575 stone Substances 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
- 239000002918 waste heat Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/20—Graphite
- C01B32/21—After-treatment
- C01B32/215—Purification; Recovery or purification of graphite formed in iron making, e.g. kish graphite
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- Life Sciences & Earth Sciences (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Geology (AREA)
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Environmental & Geological Engineering (AREA)
- Inorganic Chemistry (AREA)
- Carbon And Carbon Compounds (AREA)
Abstract
一种石墨提纯的装置和方法，涉及冶金法石墨提纯领域。一种石墨提纯的装置包括低温反应性离子气体发生器、流化床反应器、产品收集器、高温加热区和气固分离器；石墨原料通过产品收集器内部的热交换管道后进入流化床反应器，反应性离子气体经低温反应性离子气体发生器离化后进入流化床反应器并与原料石墨中的杂质进行反应，废气经气固分离器进入废气回收器内净化，惰性气体从废气回收器输出后循环使用；同时，气固分离器中的石墨进入高温加热区进行高温提纯；高温提纯后的石墨进入产品收集器并与原料石墨进行热交换。采用低温反应性离子气体结合流化床工艺，从而实现低能耗、低污染、低成本的石墨洁净冶炼提纯。
A graphite purification device and method relate to the field of metallurgical graphite purification. A graphite purification device includes a low temperature reactive ion gas generator, a fluidized bed reactor, a product collector, a high temperature heating zone and a gas-solid separator; the graphite raw material enters the fluidized bed reaction after passing through a heat exchange pipe inside the product collector The reactive ion gas is ionized by the low-temperature reactive ion gas generator and then enters the fluidized bed reactor and reacts with the impurities in the raw graphite. After the recycler is output, it is recycled; at the same time, the graphite in the gas-solid separator enters the high-temperature heating zone for high-temperature purification; the graphite after high-temperature purification enters the product collector and exchanges heat with the raw graphite. The low-temperature reactive ion gas is combined with the fluidized bed process to achieve clean smelting and purification of graphite with low energy consumption, low pollution and low cost.
Description
Technical field
The present invention relates to metallurgy method graphite purification field more particularly to a kind of device and method of graphite purification.
Background technique
Graphite resource is classified as key raw material by many countries, plays extremely in industry and the national economic development
Important role.Planning of science activities, orderly development are to guarantee graphite industry sustainable development and form good economic benefits and society
The important prerequisite of benefit.The purification of graphite is the basis for preparing all graphite materials, is the common problem of graphite material development.It is existing
Some graphite purification methods include: (1) alkali acid system, and alkali acid system can get the graphite products of fixed 99% or more carbon content, but dirty
Dye is serious；(2) hydrogen fluoride or mixed acid process, such method can get purity 99.9% graphite, but hydrofluoric acid have severe toxicity and
Strong corrosive, Environmental Inputs are big；(3) chlorinating roasting can get the graphite products that purity is greater than 98%, but tail gas difficulty
Reason, seriously polluted, severe corrosion to equipment, and chlorine is at high cost；(4) floatation, floatation can get purity 90~98%
Graphite concentrate, further there is still a need for utilize chemical method or high temperature method for purification；(5) high temperature method can get 99.99% or more purity
Ultra-pure graphite, but equipment is expensive, one-time investment is more, energy consumption is high.Therefore, a kind of low energy consumption, low pollution, low cost stone
Black clean smelting method of purification has important real value and war to China's graphite quality and the manufacture of high-end graphite products is promoted
Slightly meaning.
Chinese patent CN101817523B discloses a kind of graphitizable high temperature vertical continuous induction heating furnace, a vertical circle
The burner hearth of cylinder space, burner hearth top connect feeding device, connect discharging device below burner hearth, pass through 3000 DEG C of height of highest
Temperature makes impurity gasification volatilization.Although the purpose of high temperature method purification may be implemented in the patent, but it is still not energy saving enough, and impurity
Gas discharge will cause a degree of environmental pollution.
Chinese patent CN103172060B is disclosed is segmented downwards the inclined long cylinder of closing using one from high to low
As high temperature purification main body, feed zone, feed surge area, low-temperature heat are in turn divided into low side since high-end in long cylinder
Area, medium temperature heating zone, high-temperature heating area, clinker buffer area and the material discharge region that cools, can produce 99%, 99.9%, 99.99%
High-purity microlite ink powder, and devise by-product plant, but it is 2700 DEG C that it, which purifies temperature, cannot accomplish low temperature, low
Energy consumption.
Summary of the invention
It is an object of the invention to solve the above problem in the prior art, device and the side of a kind of graphite purification are provided
Method is made graphite miberal powder under fluidized state, is passed through reactive ion using low-temp reaction ionized gas combination fluidized-bed process
Gas.It because of the specific very high activity of reactive ion gas, can be chemically reacted with the impurity in graphite, generate low boiling point
Compound, and separate low-boiling compound with graphitic carbon particles, to realize that low energy consumption, low pollution, the graphite of low cost are clean
It is net to smelt purification.
In order to achieve the above objectives, the present invention adopts the following technical scheme:
A kind of device of graphite purification, including raw material memory, axis are anti-from blower, gas reservoir, preheating assembly, low temperature
Answering property ionized gas generator, fluidized-bed reactor, gas-solid separator；
Raw material memory is for storing graphite raw material；
Gas reservoir is for storing inert gas；
Input terminal of the axis from blower is connect with gas reservoir pipeline, output end of the axis from blower and raw material pipeline memory
Connection, axis is from blower for blowing gas to convey graphite raw material；
The input terminal of fluidized-bed reactor is connect with raw material pipeline memory, the output end of fluidized-bed reactor and gas-solid point
Input terminal pipeline connection from device；
Preheating assembly is set to the input terminal of fluidized-bed reactor, and preheating assembly is for carrying out graphite raw material to be heated to target
Temperature；
Low-temp reaction ionized gas generator is connect with fluidized-bed reactor pipeline, and low-temp reaction ionized gas occurs
Device after reactive ion gas ionization for will be transported in fluidized-bed reactor.
The invention also includes waste gas recovery device and driers；Waste gas recovery device is provided with the solvent for dissolving exhaust gas, gas
The pipeline at output of solid separator protrudes into solvent, and the output end and axis of waste gas recovery device are connected from blower with will be purified lazy
Property gas is transported to axis from blower to be recycled again；The drier is set to waste gas recovery device and axis between blower.
Filtering baffle is equipped in the gas-solid separator, the pipeline at output of fluidized-bed reactor is connected under filtering baffle
Side, the pipeline at output of gas-solid separator are connected to the top of filtering baffle.
It is additionally provided with high temperature purification device below the gas-solid separator, the inside of high temperature purification device is from top to bottom successively
Equipped with high-temperature heating area and product collector；The input terminal in the high-temperature heating area connects gas-solid separator, and high-temperature heating area uses
High temperature purification is carried out in the graphite for separating gas-solid separator；Product collector is used to collect the height produced from high-temperature heating area
Pure graphite.
It include heat exchanging pipe in the pipeline of present invention connection fluidized-bed reactor and raw material memory, the heat exchange
Pipeline runs through product collector.
The invention also includes high-temp waste gas depositor, the input terminal of the high-temp waste gas depositor connects high temperature purification device
Top, the output end of high-temp waste gas depositor connects waste gas recovery device.
In high temperature purification device, the high-temperature heating area is equipped with buffer part, and the buffer part is spiral channel, layering
Inclined plate or layering funnel.
A kind of method of graphite purification, using following steps:
Step 1, graphite raw material are exported from raw material memory, are blown and are conveyed from blower by axis, inside product collector
The laggard fluidized bed reactor of heat exchanging pipe, graphite raw material be heated to target temperature by preheating assembly, reactivity from
Sub- gas through the laggard fluidized bed reactor of low-temp reaction ionized gas generator ionization and with the impurity in raw graphite into
Row reaction generates low-boiling compound and higher-boiling compound；
Step 2, the graphite after fluidized-bed reactor reacts enter gas-solid separator, the exhaust gas with low-boiling compound
Enter in waste gas recovery device through filtering baffle and solvent reaction, purified inert gas is after the output of waste gas recovery device through drying
The dry axis that enters of device is recycled from blower；Meanwhile the graphite in gas-solid separator enters high-temperature heating area and carries out high temperature purification,
And be volatilized to enter into higher-boiling compound in high-temp waste gas depositor and settled, inert gas is through waste gas recovery device and drying
It is recycled after device；
Graphite after step 3, high temperature purification enters product collector from high-temperature heating area and carries out hot friendship with raw graphite
It changes.
Impurity in the raw graphite includes the simple substance or oxide of Si, Fe, Al, Ca, Na, K and Mg.
The reactive ion gas includes HCl, HF and H2At least one of O；The solvent can be alkali metal carbonic acid
One or both of salting liquid and alkali hydroxide soln；The preheating assembly and high-temperature heating area can be induction heating
Or Resistant heating；The target temperature is 300~1000 DEG C, and optimum temperature is 300~500 DEG C.
Compared with the existing technology, the beneficial effect that technical solution of the present invention obtains is:
1, present invention process is simple, and fluidization and low-temp reaction ionized gas technology are organically combined, and realizes low
The impurity such as Si, Fe, Al, Ca, Na, K, Mg in natural graphite or oxide are converted to low-boiling compound under the conditions of temperature, from
And the various impurity elements in graphite ore are effectively removed, this method greatly reduces energy consumption compared with high temperature method, with chemical method phase
Than greatly reducing pollution, entire technical process realizes that low energy consumption, the continuity graphite cleaning smelting of low pollution, low cost mention
It is pure, there is very considerable market application prospect.
2, the present invention is provided with gas-solid separator, separates low-boiling compound in advance, in order to avoid high temperature generates separation, increases
Energy consumption.
3, it is heated at high temperature area and induction heating can be used in preheating assembly, induction heating is a kind of most effective hand that is rapidly heated
Section increases temperature by the self-induction of graphite particle, can substantially reduce purification energy consumption.
4, high-temperature heating area is provided with buffer part, for example uses spiral channel, can extend graphite in high-temperature heating area
Residence time, the impurity compound in graphite is made sufficiently to be volatilized, effectively further increases the purity of graphite.
5, heat exchanging pipe is equipped in product collector, the graphite waste heat after making full use of high temperature purification by graphite raw material into
Row heating, can substantially reduce the comprehensive energy consumption of total system.
6, the present invention is equipped with waste gas recovery device, and the solvent in waste gas recovery device can be carbonate solution or the alkali gold of alkali metal
Belong to one or both of hydroxide solution, the complete reactive ion gas of the oxide impurity and unreacted in graphite is equal
It can effectively be dissolved in solvent, to make entire purification process zero-emission, clean pollution-free.
7, the present invention forms closed cycle for the inert gas of conveying in whole system, enables the system to effectively run,
Efficient successional production technology is formed, and greatly reduces the consumption of inert gas.
Detailed description of the invention
Fig. 1 is the structural diagram of the present invention.
Appended drawing reference: gas reservoir 1, axis is from blower 2, raw material memory 3, preheating assembly 4, low-temp reaction ion-gas
Body generator 5, fluidized-bed reactor 6, gas-solid separator 7, filtering baffle 8, waste gas recovery device 9, solvent 10, drier 11 are high
Warm purifying plant 12 is heated at high temperature area 13, buffer part 14, product collector 15, heat exchanging pipe 16, high-temp waste gas depositor
17。
Specific embodiment
In order to be clearer and more clear technical problems, technical solutions and advantages to be solved, tie below
Drawings and examples are closed, the present invention is described in further details.
As shown in Figure 1, the present invention includes raw material memory 3, axis from blower 2, gas reservoir 1, preheating assembly 4, low temperature
Reactive ion gas generator 5, fluidized-bed reactor 6, gas-solid separator 7, waste gas recovery device 9, drier 11, high temperature purification
Device 12, high-temp waste gas depositor 17；Wherein:
Raw material memory 3 is for storing graphite raw material；
Gas reservoir 1 is for storing inert gas；
Input terminal of the axis from blower 2 is connect with 1 pipeline of gas reservoir, output end of the axis from blower 2 and raw material memory 3
Pipeline connection, axis is from blower 2 for blowing gas to convey graphite raw material；
The input terminal of fluidized-bed reactor 6 is connect with 3 pipeline of raw material memory, the output end and gas of fluidized-bed reactor 6
The input terminal pipeline of solid separator 7 connects；
Preheating assembly 4 is set to the input terminal of fluidized-bed reactor 6, and preheating assembly 4 is for graphite raw material to be heated to
Target temperature；
Low-temp reaction ionized gas generator 5 is connect with 6 pipeline of fluidized-bed reactor, low-temp reaction ionized gas hair
Raw device 5 after reactive ion gas ionization for will be transported in fluidized-bed reactor 6；
It is equipped with filtering baffle 8 in the gas-solid separator 7, the pipeline at output of fluidized-bed reactor 6 is connected to filtering baffle 8
Lower section, the pipeline at output of gas-solid separator 7 is connected to the top of filtering baffle 8；
Waste gas recovery device 9 is provided with the solvent 10 for dissolving exhaust gas, and the pipeline at output of gas-solid separator 7 protrudes into solvent
In 10, the output end and axis of waste gas recovery device 9 from blower 2 connect with by purified inert gas be transported to axis from blower 2 with
It is recycled again；
The drier 11 is set to waste gas recovery device 9 and axis between blower 2；
The high temperature purification device 12 is set to the lower section of gas-solid separator 7, and the inside of high temperature purification device 12 is from top to bottom
It is successively arranged high-temperature heating area 13 and product collector 15；The input terminal in the high-temperature heating area 13 connects gas-solid separator 7, high
Warm heating zone 13 is used to carrying out the isolated graphite of gas-solid separator 7 into high temperature purification, and high-temperature heating is equipped with buffer part 14 in area 13,
The buffer part 14 is spiral channel, the inclined plate of layering or layering funnel；Product collector 15 is for collecting from high temperature
The high purity graphite that heating zone 13 is produced；
The top of the input terminal connection high temperature purification device 12 of the high-temp waste gas depositor 17, high-temp waste gas depositor 17
Output end connect waste gas recovery device 9.
It include heat exchanging pipe 16, the heat in the pipeline of present invention connection fluidized-bed reactor 6 and raw material memory 3
It exchanges pipeline 16 and runs through product collector 15.
Fluidized-bed reactor 6 is combined with low-temp reaction ionized gas generator 5 in the present invention, be not limited to by
Fluidized-bed reactor 6 is combined with low-temp reaction ionized gas generator 5 respectively as stand-alone assembly, can also be by low temperature
Reactive ion gas generator 5 is integrated in fluidized-bed reactor 6.
The present invention in order to guarantee be heated at high temperature area 13 have preferable heating efficiency, by heating divide into Shang Qu, Zhong Qu, under
Three sections of area heating zone.
A kind of method of graphite purification, using following steps:
Step 1, graphite raw material are exported from raw material memory 3, are blown and are conveyed from blower 2 by axis, pass through product collector 15
The internal laggard fluidized bed reactor 6 of heat exchanging pipe 16, preheating assembly 4 carry out graphite raw material to be heated to target temperature,
Reactive ion gas is through the laggard fluidized bed reactor 6 of 5 ionization of low-temp reaction ionized gas generator and and raw graphite
In impurity carry out reaction and generate low-boiling compound and higher-boiling compound；
Step 2, the graphite after the reaction of fluidized-bed reactor 6 enter gas-solid separator 7, useless with low-boiling compound
Gas enters in waste gas recovery device 9 through filtering baffle 8 to react with solvent 10, and purified inert gas is exported from waste gas recovery device 9
By the dry axis that enters of drier 11 from the recycling of blower 2；Meanwhile the graphite in gas-solid separator 7 enters high-temperature heating area
13 carry out high temperature purification, and are volatilized to enter into higher-boiling compound in high-temp waste gas depositor 17 and are settled, inert gas
It is recycled after waste gas recovery device 9 and drier 11；
Graphite after step 3, high temperature purification from high-temperature heating area 13 enter product collector 15 and with heat exchanging pipe 16
The raw graphite that interior gas carries carries out heat exchange, and last high purity graphite discharges from the discharge valve of product collector 15 and is put in storage,
And the graphite raw material in heat exchanging pipe 16 uses preheating assembly in 6 inlet of fluidized-bed reactor according to the temperature after its heat exchange
4, which carry out heating, makes up to target temperature.
Impurity in the raw graphite includes the simple substance or oxide of Si, Fe, Al, Ca, Na, K and Mg.
The reactive ion gas includes HCl, HF and H2At least one of O.
The solvent 10 is one or both of alkali metal carbonate solution and alkali hydroxide soln.
The preheating assembly 4 and high-temperature heating area 13 are induction heating or Resistant heating.
The target temperature is 300~1000 DEG C, and optimum temperature is 300~500 DEG C.
Working principle of the present invention is as follows:
Natural graphite powder is exported from raw material memory 3, is blown and is conveyed from blower 2 by axis, by heat exchanging pipe 16 and is produced
High purity graphite in product collector 15 carries out heat exchange, it is preheated after natural graphite powder enter fluidized-bed reactor 6 from pipeline,
And can further be heated up by preheating assembly 4 to graphite, reactant gas is after 5 ionization of low-temp reaction ionized gas generator
Into fluidized-bed reactor 6, in fluidized-bed reactor 6, under 300~500 DEG C of cryogenic conditions, reactive ion gas is utilized
Body (such as: HCl ionized gas) in natural graphite Si, Fe, Al, Ca, Na, K, Mg simple substance or oxide react,
Middle a part generates low-boiling compound, such as SiHCl3(33 DEG C of boiling point), SiCl4(57.6 DEG C of boiling point), NaClO (boiling point 102.2
℃)、FeCl3(315 DEG C of boiling point) and AlCl3(181 DEG C of boiling point) etc. and remove, other can then generate the relatively high chlorine of boiling point
Compound, such as CaCl2(1600 DEG C of boiling point), MgCl2(1412 DEG C of boiling point), KCl (1420 DEG C of boiling point) etc., it is reacted after graphite warp
Pipeline enters gas-solid separator 7, and the exhaust gas that carry low-boiling compound is sent into waste gas recovery device 9 by pipeline through filtering baffle 8,
Waste gas recovery device 9 is equipped with solvent 10, and after waste gas recovery device 9, low-boiling compound is filtered exhaust gas, purified inert gas
Enter drier 11 through pipeline, dried gas is recycled by pipeline, and total by the adjusting carrier gas of gas reservoir 1
Amount.On the other hand, the graphite in gas-solid separator 7 enters high temperature purification device 12 through valve, the buffering being heated at high temperature in area 13
Portion 14 can slow down the downstream rate of graphite, by adjusting the heating power of heating zone, be maintained at the temperature in buffer part 14
1600 DEG C or so, so that higher-boiling compound be made to volatilize and after the cooling deposition of high-temp waste gas depositor 17, gas is returned through exhaust gas
Enter next circulation after receiving device 9 and drier 11, and the graphite after purifying enters product collector 15 and carries out heat exchange, thus
Substantially reduce energy consumption.
Embodiment 1
The present embodiment is additionally arranged at the bottom a low-temp reaction ionized gas generator 5 in existing fluidized-bed reactor 6, and
Inlet installs a dominant frequency load coil additional as preheating apparatus below fluidized-bed reactor 6；Then in fluidized bed
A gas-solid separator 7 is installed in the outlet of reactor 6, while being mounted with a waste gas recovery device 9, that is, is constituted a graphite and mentioned
Pure device.
Graphite purification is carried out using above-mentioned graphite purifying device.Firstly, the transmission gas using high-purity Ar gas as graphite,
And be passed through HCl gas through low-temp reaction ionized gas generator 5, ionization occurs for HCl gas, and with the oxidation of impurities in graphite
Object reacts, and a portion generates low-boiling compound, and another part can then generate the relatively high chloride of boiling point.Through
The exhaust gas that gas-solid separator 7 is isolated is directly entered waste gas recovery device 9.Through reaction after a period of time, in waste gas recovery device 9
It detected the impurity elements such as Si, Fe, Al, Na in solvent 10, on the other hand, obtained graphite purity is increased to from 75%
98.3%, illustrate that graphite has obtained effective purification, and realize low energy consumption, low cost, without disposal of pollutants.
Embodiment 2
The present embodiment is transformed existing small-sized high-frequency induction smelting furnace, can be heated at high temperature using graphite crucible conduct
Gas-solid separator 7, and one-in-and-one-out two-way gas pipeline is devised on graphite lid, while in graphite lid envisaged underneath
For one perforated baffle as filtering baffle 8, graphite crucible admission line is directly inserted into crucible bottom, the air inlet of admission line
Connection is built-in with the fluidized-bed reactor 6 of low-temp reaction ionized gas generator 5, and graphite crucible outlet pipe then connects exhaust gas
Recover 9
Graphite purification is carried out using the graphite purifying device of above-mentioned transformation.Firstly, being first passed through transmission gas when experiment starts
Ar is then turned on induction heating for crucible temperature and is raised to 1600 DEG C, after 30min stop heating, after cooling, take sample into
Row analysis, graphite purity are 99.95%.
Claims (10)
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| CN109721056A (en) * | 2019-02-28 | 2019-05-07 | 扬州中天利新材料股份有限公司 | The method that depth removes impurity element in high-purity silicon carbide powder |
| CN110894070A (en) * | 2019-12-06 | 2020-03-20 | 中国科学院山西煤炭化学研究所 | Device and method for continuously preparing graphite oxide |
| CN113387354A (en) * | 2021-07-26 | 2021-09-14 | 黑龙江工业学院 | Graphite purification method and purification device |
| CN113428853A (en) * | 2021-07-21 | 2021-09-24 | 上海赛瑞达新材料工程技术有限公司 | High-temperature graphite purification device |
| CN114291815A (en) * | 2022-01-07 | 2022-04-08 | 宝丰县五星石墨有限公司 | High-purity graphite purification system |
| CN114604868A (en) * | 2022-04-07 | 2022-06-10 | 杨以柯 | Graphite purification furnace |
| CN118758054A (en) * | 2024-08-29 | 2024-10-11 | 长沙有色冶金设计研究院有限公司 | A device and process for continuous graphitization of graphite negative electrode material for lithium-ion batteries |
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| CN118758054B (en) * | 2024-08-29 | 2024-11-22 | 长沙有色冶金设计研究院有限公司 | Device and process for continuously graphitizing graphite cathode material of lithium ion battery |
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